Sublimator



July 24, 1928. 1,678,442

F. A. PEARL SUBLIMATOR Filed Dec. 1, 1927 INVERITOR I 42M ATTORNEY rill retested July 24, was

nrre srrss FRANK A. PEARL, .0 NEW YORK, N. Y.

SUBLIMATOR.

Application filed December 1, 1927/ Serial No. 237,005.

This invention relates to laboratory apparatuses employed in qualitative and quantitative analysis, and more particularly in the process of sublimation.

One of the objects of: my invention is to construct a subliming apparatus designed for determining the chemical constituents, quality or quantity of 'a constituent, also for identifying substances capable of crystallization.

More particularly, my invention relates to a subliming apparatus for identifying and determining chemical constituents qualitatively and quantitatively in micro-chemical analyses without a'l ter sublimation resorting to the aid of solvents, solutions, evaporations, tiltrations or other laboratory methods which are not feasible when only a minute substance is being treated.

A further object of my invention is to pro vide a subliming apparatus constructed and arranged for exacting and accurate work; in which the temperature determining factor is entirely protected from outside influences; in which the parts and elements are easily replaceable, convenient to handle, inexpensive to manufactureand otherwise reduces the time element in obtaining definite'resuits. e

To enable others skilled in the art to more fully comprehend the underlying features and'advantages of my invention, that the same may be practiced in laboratory, scientitle and experimental work, reference is had to'the accompanying drawing showing a preferred embodiment in which.

Fig. 1 is a vertical sec ional view showing the apparatus.

Fig. 2vis a plan view or the apparatus withthe outer casing, cooler and condenser removed.

Fig. 3 is a view, partly broken away showing the means of supporting the condenser.

Fig. 4 is a detail view of the condensing chamber.

Fig. 5 ing coils.

Referring now to the drawings wherein like reference characters designate corresponding parts throughout the. several yiews, 1 designates the lower section ot anancloziing unit which is preferably of cylindrical formation, than at its open top. The upper portion of the enclosing unit consists of-a hollow substantially elliptical shell 2, the lower vertical is a detail view showing the coolbeing slightly wider at its base wall of which interfits the top of the lower section and joined thereto by ground glass surface or otherwise as indicated by numeral 21. Within the top and bottom enclosing un t, a conically shaped cooling coil 3 is provided through which cold water or other cooling medium may flow when the apparatus is in operation.

The lower section 1 is equipped with a heating chamber 6 preferably integral therewith, the upper portion of said chamber extending somewhat above the base. The heating-chamber is provided with an outlet tube 7 having an opening 8 in the end thereof, through which air is admitted as referred to in the process later to be described. The open top oi the chamber (3 is adapted to receive adisk 5 on which the material or substance 22 is placed and to which heat is to be applied. The heating chamber is equipped with supporting lugs 19 just below the top on which the cone shaped vessel 4; is positioned and upon the inner wall of which the material to be quantitatively determined, is deposited bysublimation. It will be noted that the conical vessel 4 extends for its greater portion within the cooling coil 3-whereby crystallination of the material or substance may take place." 'On the inner surface of the vessel l, lugs 20 are provided on which a glass disk' 9 may be positioned when it is desired to qualitatively determine and identify the material being heated. The heating chamber is also provided with a hollow lateral arm 1'? located within the bottom section 1 and in proximity to the disk 5, the lateral arm 17 constituting a supportv for the lower end of a thermometer 10, the upper end of said thermometer being supported as at 11 within the interior Off the upper section 2 of the enclosing unit. 'lhe apparatus supported by the divorgin or tripod legs 18 and in such manner that heat may be applied to the bottom of the heating chamber 6. lhe cooling coil 3 is provided with an inlet 16 passing through an insulated busln ing 15and auoutlet 12 passing througha similarbushing13, said inlets and outlets being located. "in the top portion of the onclosing unit 2. The top of the unit- 2 is also equipped with an exhaust outlet 14 which maybe connected to a suction pump or other means of air exhaust, not shown, so'as'to produce a vacuum within the enclosing unit.

It will thus be seen that my apparatus may Ill) is assured.

be employedboth for quantitative and qualitative work, particularly where a minute quantity of the substance is given. When employed in qualitativeexperiments, for instance, the disk 9 is utilized so that when some of the material 22 is sublimed on the lower face of the disk 9, the crystalline structure oi this material may be identified. On the other hand, when it is desired to conduct a quantitative analysis, the disk 9 is dispensed with.

Assuming that it is desired to ascertain the quantity or a certain constituent present in a definite quantity of a substance and since the temperature at which crystallization takes place is known, heat maybe applied and regulated by means of the thermometer until complete sublimation takes place on the interior of the vessel 4:. Since the weight of the vessel 4 is previously known, the difference between the combined weight oi the vessel and the sublimed mate rial may be readily determined quantitatively. It will thus be seen that by employing this apparatus, it does not become necessary to-employ a solvent or solution or follow any or the other practices or processes commonly known.

Particular attention is directed to the temperature determining factor wherein the thermometer is positioned and located within the enclosing unit, so that absolute accuracy The lower portion of the thermon'ieter is located in proximity to the material being sublimed so that the degree of heat required may be controlled. The apparatus is so constructed that the various parts are easily removable and replaceable at slight cost, and has the advantage over present apparatuses which require complete replacement, when parts are broken.

Furthermore, in my apparatus, the percentage of error is reduced materially by reason of the fact that the ratio between the quantity of the material to be determined and the vessel upon which it is sublimed is much smaller than in those apparatuses wherein the vessel to be weighed is considerably heavier than the small amount of material which is deposited. It may also be noted that when the material is weighed for quantitative determination, it is not necessary to make allowance for moisture as is necessary with other apparatuses. By the use of my apparatus, al'ter sublimation takes place, it is not necessary to re-dissolve andrecrystallize the sublimed substance as is required in other apparatuses over which my invention is an improvement.

Having shown and described my invention, what I claim as new and desire to secure by Letters Patent is: r

1. An apparatus of the class described comprising .a heating chamber, means for supporting a substance for sublimation, a

separable vessel for receiving the deposit of material sublimed from said substance when heated,separable means for cooling said vessel, and a sectional enclosing unit for said heating chamber, supporting means, vessel an-dcooling means.

2. An apparatus of the class described comprising a heating chamber, means for supporting a substance for sublimation, a separable vessel for receiving the deposit of material sublimed from said substance, separable means for cooling said vessel, a temperature indicating device, and a sectional unit for enclosing said heating chamber, supporting means, vessel, cooling means and temperature indicating device.

3. An apparatus 01 the class described comprising a heating chamber, means for supporting a substance for sublimation, a separable vessel for receiving the deposit of material sub'limed from said substance, separable means for cooling said vessel, a temperature indicating device and a sectional unit for enclosing said heating chamber, supporting means, vessel, cooling means and temperature indicating device, said unithaving an outlet whereby air may be exhausted.

a. An apparatus of the class described comprising a heating chamber, means for supporting asubstance for sublimation, a sepa able vessel above the heating chamber for receiving the deposit of material sublimed from said substance when heated, means for cooling said vessel and a sectional unit enclosing said heating chamber, vessel and cooling means.

5. An apparatus of the class described, comprising a heating chamber, means for supporting a substance for sublimation, a vessel above the heating chamber for receiving the deposit of material sublimcd from said substance when heated, means for cool- 111 said vessel, a temperature indicating de vice and a sectional unit enclosin said heating chamber, hollow vessel, cooling means and temperature indicating device.

6. An apparatus of the class described comprising a heating chamber having means for supporting a substance for sublimation, a hollow vessel above the heating chamber for receiving the deposit of material sublimed from said substance when heated, means for cooling said vessel, an enclosing unit for said heating chamber and hollow vessel anda temperature indicator located within said unit.

7. An apparatus of the class described comprising a heating chamber havingmeans for supporting a substance for sublimation, a hollow vessel rcmovably supported above the top of said chamber for receiving the deposit of material sublimed from said sub stance when heated, an enclosing unit for said heating-chamber and hollow vessel, a cooling coil supported by said unit and surrounding the hollow vessel, said unit having an outlet whereby air may be exhausted therefrom and a tempe'ature indicator located within said unit.

8. An apparatus of the class described comprising a heating chamber having means for supporting a substance for sublimation on its top, a hollow vessel removably supported by said chamber above the top for receiving the deposit of material sublimed on its inner surface, a sectional enclosing unit for said heating chamber and hollow vessel, said unit supporting a cooling coil surrounding the hollow vessel, and having an outlet whereby it may be exhausted, and a thermon'ieter positioned. within the enclosing unit, the lower end of said thermometer being located in proximity to the substance being sublimed.

9. An apparatus of the class described comprising a heating chamber having means for supporting a substance on its top, a hollow vessel removably supported above said chamber for receiving on its inner surface the deposit of material sublimed, means for supporting a disk within said hollow vessel at a point in proximity to the top of said heating chamber, an enclosing unit for said heating chamber and hollow vessel, said unit having an outlet whereby the air may be exhausted therefrom, a cooling coil sup ported by said unit and surrounding the hollow vessel, and. a thermometer located with in said unit.

10. An apparatus of the class described con'iprising a heating chamber having means for supporting a disk on its top and on which the substance for sublimation is positioned, a hollow cone shaped vessel removably mounted above the disk for receiving the deposit of material being sublimed, a sectional unit enclosing the top of the heating chamber and the hollow vessel, the top section of said unit supporting a cooling coil surrounding the hollow vessel and having an outlet whereby the air within said unit may be e-:-:hausted, said heating chamber having a hollow arm for supporting the lower end of a thermometer positioned within the unit.

11. An apparatus of the class described comprising a heating chamber having means for supporting a substance for sublimation on its top, a removable cone shaped hollow vessel positioned. above the top of said chamber and presenting a surface on the interior of which the material being sublimed is deposited, an enclosing unit for the top of said heating chamber and hollow vessel, said unit supporting a cone shaped cooling coil surrounding the hollow vessel, said unit having an outlet whereby the air therein may tom of said unit being formed with the heat ing chamber and the top of the unit on casing the cone shaped vessel, a cone shaped cooling coil supported by the top section of said unit, said top section having an out" let whereby air may be exhausted from said unit, and a thermometer within said unit, the lower end of said thermometer being positioned in proximity to the top of the heating chamber and material being sublin'ied.

13. An apparatus of the class described comprising a heating chamber having a material supporting disk on the top thereof, a removable cone shaped, hollow vessel supported on said chamber above the top and presenting a surface on the interior of which the material sublimed may be deposited, a sectional enclosing unit having a cooling coil surrounding the hollow vessel, the inlet and outlet of said coil extending through the top of said unit, a lateral, hollow arm formed with the heating chamber for supporting the lower end of a thermometer in proximity to the material being sublimed, said thermometer being located entirely within the unit.

In testimony whereof he has aiiixed his signature.

FRANK A. PEARL. 

